CN107722371A - A kind of preparation method of montmorillonite nanometer-sized composite slurry - Google Patents
A kind of preparation method of montmorillonite nanometer-sized composite slurry Download PDFInfo
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- CN107722371A CN107722371A CN201710938069.2A CN201710938069A CN107722371A CN 107722371 A CN107722371 A CN 107722371A CN 201710938069 A CN201710938069 A CN 201710938069A CN 107722371 A CN107722371 A CN 107722371A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L3/00—Compositions of starch, amylose or amylopectin or of their derivatives or degradation products
- C08L3/02—Starch; Degradation products thereof, e.g. dextrin
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Abstract
The present invention relates to a kind of preparation method of montmorillonite nanometer-sized composite slurry, belong to field of material technology.Weathered coal ball milling is taken to sieve, obtain weathered coal powder, weathered coal powder and hydrochloric acid reaction must be washed into filter cake, weigh deionized water, ammoniacal liquor, zinc stearate and washing filter cake bath heating, then stand and be cooled to room temperature, centrifuge, collect supernatant liquor and sulfuric acid is added dropwise extremely, it is still aging, filter to obtain filter residue, rinse, dry and be prepared into modified particles, weigh epoxychloropropane, diethylenetriamine and modified particles and be placed in beaker, it is stirred, filter blending filter cake and to rinse, be dried in vacuo and ball milling sieving, obtain modified powder；Modified powder and deionized water are stirred simultaneously ultrasonic disperse, collect to obtain dispersion liquid, weighing dispersion liquid, cornstarch, montmorillonite are placed in beaker, heating water bath, cooling is stood, pH is adjusted with sodium hydroxide solution, ultrasonic disperse again, you can be prepared into a kind of montmorillonite nanometer-sized composite slurry.
Description
Technical field
The present invention relates to a kind of preparation method of montmorillonite nanometer-sized composite slurry, belong to field of material technology.
Background technology
With making rapid progress for modern science and technology, extensive and harsh, list of the people to material requirement also increasingly
The material of one component has generally been difficult to the needs for meeting society.Two or more heterogeneous, special-shaped, different in nature material is led to
Certain technique groups synthetic composite material is crossed, meets the expected requirement of people's performance in terms of certain, it has also become exploitation high-performance material
The important channel of material.It can be said that the Composite of material is the main trend of current materials industry development.It is compound can be understood as it is micro-
See the interaction of all systems on yardstick.Traditional composite be by the use of particle, whisker, fiber of pin level etc. as filler,
For improving the mechanical property of material；And nano composite material refers to that dispersed phase yardstick is at least one-dimensional compound less than 100nm
Material, because nano material has four big characteristics:Nanometer size effect, surface-interface effect, quantum size effect and macroscopical tunnel
Channel effect, this causes nano composite material to have traditional material unrivaled excellent in mechanics, calorifics, electrical and optical etc.
Gesture, have broad application prospects.This also makes a focus and emphasis of the nano material as this century material science research.It is poly-
Compound nano composite material is using polymer as matrix, and the organic inorganic nano using various inorganic nano-fillers as dispersed phase is answered
Condensation material.Montmorillonite is a kind of clay mineral of China's high yield, belongs to 2：The stratiform or sheet silicate mineral of l types, i.e. two layers of silicon
One layer of alumina octahedral chip Component units crystal layer of folder among oxygen tetrahedron chip, its crystal layer thickness about 1nm, planar dimension is about
100nm.Montmorillonite crystal layer is up and down oxygen atom, and hydrone causes lattice dilatation between being easily accessible crystal layer, in its lattice knot
Some metallic atoms are substituted by other different metallic atoms of chemical valence in structure, although its lattice framework keeps constant, crystal
Lamella generates negative electrical charge, and the cation in the adsorbable surrounding medium of the negative electrical charge reaches charge balance, in aqueous, aquation
Cation enter between crystal layer, cause its interlamellar spacing to become big, thus it can with various organic cations (such as alkylammonium from
Son/cationic surfactant) the original hydrated cation of its interlayer replaced by ion-exchange reactions, so that generally parent
The montmorillonite of water is surface-hydrophobicized, and its exchange rate is related to unsaturated cationic chemical valence and intercalator species.When interlamellar spacing increases
To more than during molecular separating force sphere of action, montmorillonite occurs disintegration and peeled off, and generates lamellar spacing about 1nm inorganic receiving between crystal layer
Rice corpuscles.Tradable cation number is that cation exchange capacity (CEC) is macromolecule success intercalation between inorganic layer
One important indicator.For PLS nano composite materials, the optimum CEC of phyllosilicate should be 90~120meq/
100g, this is exactly CEC values possessed by montmorillonite.If CEC values are too high, inorganic matter piece interlayer Coulomb force will be caused excessive, it is unfavorable
In the insertion of macromolecular chain；If otherwise CEC values are too low, prevent again inorganic matter from effectively with interpolymer interaction, it is difficult to protect
Demonstrate,prove the compatible of inorganic matter and polymeric matrix.Montmorillonite because its ion exchange capacity is moderate, good mechanical performance, it is cheap and
As the preferred mineral of preparation nano composite material.
The content of the invention
The technical problems to be solved by the invention：For after slurry film forming, slurry film is not tough enough the problem of, there is provided one
The preparation method of kind montmorillonite nanometer-sized composite slurry.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
Specifically preparation process is：
（1）Take weathered coal and ball milling crosses 200 mesh sieves, obtain weathered coal powder, in mass ratio 1：10, weathered coal powder is stirred with hydrochloric acid
Mix and mix and stand activation, filter filter cake and to wash, obtain washing filter cake；
（2）Count in parts by weight, weigh 45~50 parts of deionized waters, 10~15 parts of ammoniacal liquor, 1~2 part of zinc stearate and 10 respectively
~15 parts of washing filter cake heating water baths, standing are cooled to room temperature, centrifuge and collect supernatant liquor, dropwise addition sulfuric acid to pH to 2.0,
After still aging, filter residue is filtered to obtain, washing, drying are prepared into modified particles；
（3）Count in parts by weight, weigh 45~50 parts of epoxychloropropane, 20~30 parts of diethylenetriamines and 6~8 parts of modifications respectively
Particle is stirred, filter blending filter cake and wash, dry, ball milling, sieving, obtain modified powder；
（4）In mass ratio 1:25, modified powder and deionized water are stirred, ultrasonic disperse, collect to obtain dispersion liquid, by weight
Number meter, respectively 45~50 parts of dispersion liquids of weighing, 10~15 parts of cornstarch, 6~8 part of 200 mesh montmorillonite are stirred, water-bath
Heat and stand cooling, adjust pH to 7.0, ultrasonic disperse, you can be prepared into a kind of montmorillonite nanometer-sized composite slurry.
Step（2）Described ammoniacal liquor is the ammonia spirit of mass fraction 10%.
Step（4）Described regulation pH is using the sodium hydroxide solution of mass fraction 1%.
Compared with other method, advantageous effects are the present invention：
The present invention is that raw material carries out extracting nanometer humic acid by weathered coal, by nanometer humic acid, then passes through nanometer humic acid
Mixed with epoxychloropropane inexpensive, by the crosslinking humic acid of preparation, effectively strengthen active group amount in humic acid effect, improve it
Absorption property, because the silicon surface properties contained inside montmorillonite are hydrophobic, not hydroxyl, inactive, and aluminium face carries and is on a small quantity
Weakly acidic hydroxyl, lateral margin carry part silanol group and mistrimmed Al3+, pass through humic acid and montmorillonite Composite, humic acid
Molecule is sporadicly distributed on the avtive spot of kaolin surface first, with the increase of content of humic acid, part humic acid molecule
Into the hole of kaolin surface, reach after stablizing relatively, humic acid molecule continues and kaolin surface avtive spot phase mutual connection
Touch and form first layer humic acid molecular film, effectively cover montmorillonite material and improve its film strength, be effectively improved its hygroscopicity
Can, intensity greatly enhances after making its film forming.
Embodiment
Take weathered coal and ball milling crosses 200 mesh sieves, obtain weathered coal powder, in mass ratio 1：10, by weathered coal powder and quality
The hydrochloric acid of fraction 5% is stirred and stands 2~3h of activation, filters to obtain filter cake and with deionized water rinsing 3~5 times, must wash filter
Cake, count in parts by weight, weigh 45~50 parts of deionized waters, 10~15 parts of ammoniacal liquor of mass fraction 10%, 1~2 part of tristearin respectively
Sour zinc and 10~15 parts of washing filter cakes are placed in 2~3h of heating water bath at 45~50 DEG C, then stand and are cooled to room temperature, 1500~
10~15min is centrifuged under 1800r/min, supernatant liquor is collected and the sulfuric acid of mass fraction 10% is added dropwise to pH to 2.0, stand
After being aged 6~8h, filter residue is filtered to obtain, after deionized water rinsing 3~5 times, vacuum drying is prepared into modified particles, by weight
Number meter, 45~50 parts of epoxychloropropane, 20~30 parts of diethylenetriamines and 6~8 parts of modified particles are weighed respectively and are placed in beaker,
Be stirred 10~15min, filter blending filter cake and with absolute ethyl alcohol rinse 3~5 times, be dried in vacuo and ball milling cross 200 mesh
Sieve, obtains modified powder；In mass ratio 1:25, modified powder and deionized water are stirred and are placed in ultrasound under 200~300W
Scattered 10~15min, collects to obtain dispersion liquid, counts in parts by weight, weighs 45~50 parts of dispersion liquids respectively, 10~15 parts of corns form sediment
Powder, 6~8 part of 200 mesh montmorillonite are placed in beaker, and at 85~90 DEG C after 2~3h of heating water bath, standing is cooled to 45~60
DEG C, pH is adjusted to 7.0 with the sodium hydroxide solution of mass fraction 1%, then 10~15min of ultrasonic disperse under 200~300W, you can
It is prepared into a kind of montmorillonite nanometer-sized composite slurry.
Example 1
Take weathered coal and ball milling crosses 200 mesh sieves, obtain weathered coal powder, in mass ratio 1：10, by weathered coal powder and mass fraction
5% hydrochloric acid is stirred and stands activation 2h, filters to obtain filter cake and with deionized water rinsing 3 times, obtains washing filter cake, by weight
Number meter, 45 parts of deionized waters, 10 parts of ammoniacal liquor of mass fraction 10%, 1 part of zinc stearate and 10 parts of washing filter cakes are weighed respectively and are placed in
Heating water bath 2h at 45 DEG C, then stand and be cooled to room temperature, 10min is centrifuged under 1500r/min, collect supernatant liquor simultaneously
The sulfuric acid of mass fraction 10% is added dropwise to pH to 2.0, after still aging 6h, filters to obtain filter residue, after deionized water rinsing 3 times, very
Sky drying is prepared into modified particles, counts in parts by weight, respectively 45 parts of epoxychloropropane of weighing, 20 parts of diethylenetriamines and 6 parts
Modified particles are placed in beaker, are stirred 10min, filter blending filter cake and with absolute ethyl alcohol rinse 3 times, vacuum drying simultaneously
Ball milling crosses 200 mesh sieves, obtains modified powder；In mass ratio 1:25, modified powder and deionized water are stirred and are placed in 200W
Lower ultrasonic disperse 10min, collects to obtain dispersion liquid, counts in parts by weight, respectively weigh 45 parts of dispersion liquids, 10 parts of cornstarch, 6 parts
200 mesh montmorillonites are placed in beaker, and at 85 DEG C after heating water bath 2h, standing is cooled to 45 DEG C, with the hydroxide of mass fraction 1%
Sodium solution adjusts pH to 7.0, then the ultrasonic disperse 10min under 200W, you can is prepared into a kind of montmorillonite nanometer-sized composite slurry.
Example 2
Take weathered coal and ball milling crosses 200 mesh sieves, obtain weathered coal powder, in mass ratio 1：10, by weathered coal powder and mass fraction
5% hydrochloric acid is stirred and stands activation 2h, filters to obtain filter cake and with deionized water rinsing 4 times, obtains washing filter cake, by weight
Number meter, 47 parts of deionized waters, 13 parts of ammoniacal liquor of mass fraction 10%, 1 part of zinc stearate and 13 parts of washing filter cakes are weighed respectively and are placed in
Heating water bath 2h at 47 DEG C, then stand and be cooled to room temperature, 12min is centrifuged under 16500r/min, collect supernatant liquor
And the sulfuric acid of mass fraction 10% is added dropwise to pH to 2.0, and after still aging 7h, filter residue is filtered to obtain, after deionized water rinsing 4 times,
Vacuum drying is prepared into modified particles, counts in parts by weight, weighs 47 parts of epoxychloropropane, 25 parts of diethylenetriamines and 7 respectively
Part modified particles are placed in beaker, are stirred 12min, filter blending filter cake and to be rinsed 4 times with absolute ethyl alcohol, vacuum drying
And ball milling crosses 200 mesh sieves, obtains modified powder；In mass ratio 1:25, modified powder is stirred with deionized water and is placed in
Ultrasonic disperse 13min under 250W, dispersion liquid is collected to obtain, is counted in parts by weight, weigh 47 parts of dispersion liquids respectively, 13 parts of corns form sediment
Powder, 7 part of 200 mesh montmorillonite are placed in beaker, and at 87 DEG C after heating water bath 2h, standing is cooled to 52 DEG C, with mass fraction 1%
Sodium hydroxide solution adjusts pH to 7.0, then the ultrasonic disperse 13min under 250W, you can it is compound to be prepared into a kind of montmorillonite-based nano
Slurry.
Example 3
Take weathered coal and ball milling crosses 200 mesh sieves, obtain weathered coal powder, in mass ratio 1：10, by weathered coal powder and mass fraction
5% hydrochloric acid is stirred and stands activation 3h, filters to obtain filter cake and with deionized water rinsing 5 times, obtains washing filter cake, by weight
Number meter, 50 parts of deionized waters, 15 parts of ammoniacal liquor of mass fraction 10%, 2 parts of zinc stearates and 15 parts of washing filter cakes are weighed respectively and are placed in
Heating water bath 3h at 50 DEG C, then stand and be cooled to room temperature, 15min is centrifuged under 1800r/min, collect supernatant liquor simultaneously
The sulfuric acid of mass fraction 10% is added dropwise to pH to 2.0, after still aging 8h, filters to obtain filter residue, after deionized water rinsing 5 times, very
Sky drying is prepared into modified particles, counts in parts by weight, respectively 50 parts of epoxychloropropane of weighing, 30 parts of diethylenetriamines and 8 parts
Modified particles are placed in beaker, are stirred 15min, filter blending filter cake and with absolute ethyl alcohol rinse 5 times, vacuum drying simultaneously
Ball milling crosses 200 mesh sieves, obtains modified powder；In mass ratio 1:25, modified powder and deionized water are stirred and are placed in 300W
Lower ultrasonic disperse 15min, collects to obtain dispersion liquid, counts in parts by weight, respectively weigh 50 parts of dispersion liquids, 15 parts of cornstarch, 8 parts
200 mesh montmorillonites are placed in beaker, and at 90 DEG C after heating water bath 3h, standing is cooled to 60 DEG C, with the hydroxide of mass fraction 1%
Sodium solution adjusts pH to 7.0, then the ultrasonic disperse 15min under 300W, you can is prepared into a kind of montmorillonite nanometer-sized composite slurry.
The composite mortar that a kind of montmorillonite nanometer-sized composite slurry being prepared into and Heilungkiang company produce is detected,
Specific detection is as follows：
（1）The ultimate strength and test of elongation rate of serous coat
Serous coat is cut into the wide 10mm bar-shaped samples of long 220mm, thermostatic constant wet chamber's inner equilibrium is placed on 24 hours, then in YG061 types
Its ultimate strength and elongation at break (sample holder distance 100mm, decrease speed are tested on full-automatic electronic single yarn tester
50In/min), every kind of serous coat is tested 10 times, calculates its average value.
（2）The hygroscopicity test of serous coat
1g serous coat is weighed, is cut into small pieces, is placed in after baking oven is dried to adiabatic drying, claims its dry weight；Then in 65% phase
To being balanced one week under humidity, then claim the weight after its moisture absorption, substitute into following equation and calculate:
The hydroscopicity (%) of serous coat=(dry weight of weight one after moisture absorption)/dry weight × 100%
（3）The viscosity test of slurry
Nano combined slurries 100ml is configured, takes pure cotton, polyester-cotton blend, rove takes out, spontaneously dried in 95 DEG C of soaking paste 5min.
The type fabric strength machines (Tectile Machinery Plant No. 2, Changzhou City) of YC026 1 according to rove method [6#) tested.Test number (TN) is
10, take its average value.Specific test result such as table 1
The montmorillonite nanometer-sized composite slurry performance characterization of table 1
As shown in Table 1, the montmorillonite nanometer-sized composite slurry that the present invention is prepared into, ultimate strength and elongation at break all obtain substantially
Improve, hydroscopicity increase, adhesion weakens, had broad application prospects.
Claims (3)
1. a kind of preparation method of montmorillonite nanometer-sized composite slurry, it is characterised in that specifically preparation process is：
（1）Take weathered coal and ball milling crosses 200 mesh sieves, obtain weathered coal powder, in mass ratio 1：10, weathered coal powder is stirred with hydrochloric acid
Mix and mix and stand activation, filter filter cake and to wash, obtain washing filter cake；
（2）Count in parts by weight, weigh 45~50 parts of deionized waters, 10~15 parts of ammoniacal liquor, 1~2 part of zinc stearate and 10 respectively
~15 parts of washing filter cake heating water baths, standing are cooled to room temperature, centrifuge and collect supernatant liquor, dropwise addition sulfuric acid to pH to 2.0,
After still aging, filter residue is filtered to obtain, washing, drying are prepared into modified particles；
（3）Count in parts by weight, weigh 45~50 parts of epoxychloropropane, 20~30 parts of diethylenetriamines and 6~8 parts of modifications respectively
Particle is stirred, filter blending filter cake and wash, dry, ball milling, sieving, obtain modified powder；
（4）In mass ratio 1:25, modified powder and deionized water are stirred, ultrasonic disperse, collect to obtain dispersion liquid, by weight
Number meter, respectively 45~50 parts of dispersion liquids of weighing, 10~15 parts of cornstarch, 6~8 part of 200 mesh montmorillonite are stirred, water-bath
Heat and stand cooling, adjust pH to 7.0, ultrasonic disperse, you can be prepared into a kind of montmorillonite nanometer-sized composite slurry.
A kind of 2. preparation method of montmorillonite nanometer-sized composite slurry according to claim 1, it is characterised in that：Step（2）
Described ammoniacal liquor is the ammonia spirit of mass fraction 10%.
A kind of 3. preparation method of montmorillonite nanometer-sized composite slurry according to claim 1, it is characterised in that：Step（4）
Described regulation pH is using the sodium hydroxide solution of mass fraction 1%.
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Citations (4)
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|---|---|---|---|---|
| CN1250064A (en) * | 1998-10-06 | 2000-04-12 | 中国科学院化学研究所 | Preparation of epoxy resin/montmorillonoid intercalation composite material |
| CN1354198A (en) * | 2001-12-26 | 2002-06-19 | 河北工业大学 | Epoxy resin/montmorillonoid nano-compoiste-material and its preparation method |
| CN102146197A (en) * | 2011-04-20 | 2011-08-10 | 东华大学 | Method for preparing nanomontmorillonite intercalated epoxy resin exfoliated composite material |
| CN106243636A (en) * | 2016-08-02 | 2016-12-21 | 安徽美翔塑业有限公司 | A kind of starch novolac epoxy resin is blended degradable sealing bag and preparation method thereof |
-
2017
- 2017-10-11 CN CN201710938069.2A patent/CN107722371A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1250064A (en) * | 1998-10-06 | 2000-04-12 | 中国科学院化学研究所 | Preparation of epoxy resin/montmorillonoid intercalation composite material |
| CN1354198A (en) * | 2001-12-26 | 2002-06-19 | 河北工业大学 | Epoxy resin/montmorillonoid nano-compoiste-material and its preparation method |
| CN102146197A (en) * | 2011-04-20 | 2011-08-10 | 东华大学 | Method for preparing nanomontmorillonite intercalated epoxy resin exfoliated composite material |
| CN106243636A (en) * | 2016-08-02 | 2016-12-21 | 安徽美翔塑业有限公司 | A kind of starch novolac epoxy resin is blended degradable sealing bag and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| 刘静欣等: "交联腐殖酸CHA对水体中铅的吸附性能", 《环境工程学报》 * |
| 曲海滨等: "腐植酸复肥生产中风化煤腐植酸化学活化条件分析", 《磷肥与复肥》 * |
| 朱洪法: "《环境保护辞典》", 30 June 2009, 金盾出版社 * |
| 王飞龙等: "淀粉蒙脱土复合浆料的制备及性能测试", 《棉纺织技术》 * |
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Application publication date: 20180223 |